Ansa group 4 metal bis ( mu -substituted) aluminum complexes
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example 1
Reaction of (t-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitanium dimethyl with two equivalents of tris(pentafluorophenyl)aluminum ##STR9##
NMR reactions were carried out in J-Young NMR tubes or NMR tubes with good seals, and the samples were loaded into the NMR tubes in a glove box after mixing the above two reagents ((t-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitanium dimethyl and FAAL) in 0.7 mL of benzene-d.sub.6 in a 1:2 ratio (0.02 mmol scale). The mixture was allowed to react at room temperature for 20 min before the NMR spectra were recorded. An orange solution was observed and the NMR data are consistent with the structure shown in the above equation. This species has a half-life of about 2.5 h at room temperature.
Spectroscopic data for Me.sub.2 Si(.eta..sup.5 -Me.sub.4 C.sub.5)(t-BuN)Ti[(.mu.-Me)Al(C.sub.6 F.sub.5).sub.3 ].sub.2 are as folllows. .sup.1 H NMR (C6D.sub.6, 23.degree. C.): .delta. 1.61 (s, 6 H, C.sub.5 Me.sub.4), 1.49 (s, 6 H, C.sub.5 ...
example 2
Reaction of (t-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitanium dimethyl with two equivalents of tris(pentafluorophenyl)aluminum, 24 hour study ##STR10##
NMR reactions were carried out in J-Young NMR tubes or NMR tubes with good seals, and the samples were loaded into the NMR tubes in a glove box after mixing the above two reagents ((t-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitaniu m dimethyl and FAAL) in 0.7 mL of benzene-d.sub.6 in a 1:2 ratio (0.02 mmol scale). The mixture was allowed to react at room temperature and the reaction was monitored by NMR measurements. The initially formed bis(.mu.-methyl) species Me.sub.2 Si(.eta..sup.5 -Me.sub.4 C.sub.5)(t-BuN)Ti[(.mu.-Me)Al(C.sub.6 F.sub.5).sub.3 ].sub.2 was slowly converted over 24 hours in quantitative yield to two species Me.sub.2 Si(.eta..sup.5 -Me.sub.4 C.sub.5)(t-BuN)Ti(C.sub.6 F.sub.5)(.mu.-Me)Al(C.sub.6 F.sub.5).sub.3 and [(C.sub.6 F.sub.5).sub.2 AlMe].sub.2 shown in the above equation.
Spectrosco...
example 3
Reaction of (n-butylamido)dimethyl(tetramethylcyclopentadienyl)silanetitanium dimethyl with two equivalents of tris(pentafluorophenyl)aluminum ##STR11## A. Preparation of N-n-butylamino(dimethyl)tetramethylcyclopentadienylsilane
To a solution of 7.06 g (32.9 mmol) of chloro(dimethyl)tetramethylcyclopentadienylsilane in about 100 mL of hexane was slowly added about 8.0 mL (5.9 g, 8.1 mmol) of n-butylamine. Voluminous precipitate formed immediately. The reaction mixture was stirred overnight, filtered, the solids were extracted with hexane, and the volatiles were removed from the combined filtrates to give a pale yellow liquid. Yield: 8.09 g, 97.8 percent.
.sup.1 H NMR (C.sub.6 D.sub.6): d 2.83 (s, 1H, NH), 2.63 (q, J=6.7 Hz, 2H, CH.sub.2), 1.99 (s, 6H, C.sub.5 Me.sub.4), 1.85 (s, 6H, C.sub.5 Me.sub.4), 1.25 (br m, 4H, CH.sub.2 CH.sub.2), 0.88 (t, J=6.9 Hz, 3H, CH.sub.3), 0.17 (s, 1H, SiCH), 0.01 (s, 6H, SiMe.sub.2). .sup.13 C (C.sub.6 D.sub.6): d 135.4, 132.8, 56.9, 42.1, 37.4, 20.5, 1...
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